Title:
Closed, heated reaction chamber design for dynamic high-temperature x-ray- diffraction analyses of gas/solid displacement reactions
Closed, heated reaction chamber design for dynamic high-temperature x-ray- diffraction analyses of gas/solid displacement reactions
Files
Author(s)
Haluska, Michael S.
Snyder, Robert L.
Sandhage, Kenneth H.
Misture, Scott T.
Snyder, Robert L.
Sandhage, Kenneth H.
Misture, Scott T.
Advisor(s)
Editor(s)
Collections
Supplementary to
Permanent Link
Abstract
A closed, x-ray transparent chamber for containing a hot reactive gas (generated from an internal condensed source) has been designed and evaluated for use in dynamic x-ray-diffraction analysis of a gas/solid displacement reaction. The chamber consisted of a square-bottom base and lid machined from dense pyrolytic graphite. The base contained a flat pedestal, upon which SiO₂ microshells (the reactant oxide) were placed, raised above adjacent cavities holding Mg flakes (the condensed precursor to the reactive gas). Upon heating to 650 °C, the Mg evaporated and reacted with the SiO₂ inside the sealed chamber. By passing incident and diffracted x rays through the vertical side walls of the chamber and by blocking undesired graphite-diffracted x rays with platinum, the Mg(g)/SiO₂(s) displacement reaction could be tracked with time. This is the first use of dynamic high-temperature x-ray diffraction analysis to monitor the progress of a displacement reaction involving a reactant gas that was generated and confined within a closed reaction chamber.
Sponsor
Date Issued
2005-12
Extent
Resource Type
Text
Resource Subtype
Article